Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS
Autor(a) principal: | |
---|---|
Data de Publicação: | 2016 |
Tipo de documento: | Tese |
Idioma: | por |
Título da fonte: | Manancial - Repositório Digital da UFSM |
Texto Completo: | http://repositorio.ufsm.br/handle/1/17600 |
Resumo: | Antibiotics have been widely used for prophylactic and therapeutic treatment within the broiler supply chain in order to improve animal production performance. The indiscriminate use of these drugs can, however, lead to the presence of residues in the meat and thus be a risk to the health of consumers. Fluoroquinolones and tetracyclines are two antibiotic classes that are commonly used in poultry. In this study, a liquid chromatography-based analytical method coupled with mass spectrometry was developed and validated in order to analyze residues of 7 antibiotics from the aforementioned classes in chicken muscle. Furthermore, antibiotic depletion studies were performed in broiler chickens in order to quantify the residues in the meat. The results were compared to maximum residue limits (MRLs) established by Brazilian and international laws. A procedure that employs acidified acetonitrile and purification by centrifugation and low temperature precipitation was used as the extraction method, with no need to perform a solid phase extraction (SPE) step. The method was validated in accordance with the Directive 2002/657/EC from the European Union by assessing selectivity, linearity and specificity parameters, detection and quantification limits, accuracy, precision, matrix effect, decision limit (CCα), detection capability (CCβ), robustness and applicability of the technique. For depletion studies, chlortetracycline (CTC), doxycycline (DOX) and oxytetracycline (OTC) were administered orally for 5 consecutive days and ciprofloxacin (CIP), enrofloxacin (ENR) and norfloxacin (NOR) for 3 days. After 6, 12, 24, 48, 72, 96, 120, 144, 168, 192, 216 and 240 h after the last dose, muscle samples (chest) were collected from 4 animals from each treated group and from 2 from the control group in order to assess the residual concentration of the drugs. The validated method presented values within acceptable parameters according to Directive 2002/657/EC. From 65 chicken muscle samples evaluated for the applicability parameter, 3 presented residues of ENR. In the tetracyclines depletion studies, results showed that residues were under the MRLs considering Brazilian and European laws after 1 day for CTC and after 3 days for DOX. For OCT, this period was of 2 and 3 days according to Brazilian and European laws respectively. According to Japanese law, withdrawal time of 1, 5 and 2 days would be needed for CTC, DOX and OCT respectively. In the fluoroquinolones study, it was possible to detect traces of ENR even 9 days after treatment, which would make the export of meat to the United States and Canada infeasible. After 1 day at the last dose administrated, CIP residues were under MRLs established by Brazilian, European and Japanese laws, and after 4 days they were under limits determined by the Unites States and Canada. In the case of NOR, the withdrawal time would be of 1 day for all countries mentioned here. The results presented cooperate with the pursuit of food safety to consumers, as well as with the employment of analytical methods capable of determining drugs to comprise residue depletion studies in broilers. |
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2019-07-29T20:40:21Z2019-07-29T20:40:21Z2016-03-11http://repositorio.ufsm.br/handle/1/17600Antibiotics have been widely used for prophylactic and therapeutic treatment within the broiler supply chain in order to improve animal production performance. The indiscriminate use of these drugs can, however, lead to the presence of residues in the meat and thus be a risk to the health of consumers. Fluoroquinolones and tetracyclines are two antibiotic classes that are commonly used in poultry. In this study, a liquid chromatography-based analytical method coupled with mass spectrometry was developed and validated in order to analyze residues of 7 antibiotics from the aforementioned classes in chicken muscle. Furthermore, antibiotic depletion studies were performed in broiler chickens in order to quantify the residues in the meat. The results were compared to maximum residue limits (MRLs) established by Brazilian and international laws. A procedure that employs acidified acetonitrile and purification by centrifugation and low temperature precipitation was used as the extraction method, with no need to perform a solid phase extraction (SPE) step. The method was validated in accordance with the Directive 2002/657/EC from the European Union by assessing selectivity, linearity and specificity parameters, detection and quantification limits, accuracy, precision, matrix effect, decision limit (CCα), detection capability (CCβ), robustness and applicability of the technique. For depletion studies, chlortetracycline (CTC), doxycycline (DOX) and oxytetracycline (OTC) were administered orally for 5 consecutive days and ciprofloxacin (CIP), enrofloxacin (ENR) and norfloxacin (NOR) for 3 days. After 6, 12, 24, 48, 72, 96, 120, 144, 168, 192, 216 and 240 h after the last dose, muscle samples (chest) were collected from 4 animals from each treated group and from 2 from the control group in order to assess the residual concentration of the drugs. The validated method presented values within acceptable parameters according to Directive 2002/657/EC. From 65 chicken muscle samples evaluated for the applicability parameter, 3 presented residues of ENR. In the tetracyclines depletion studies, results showed that residues were under the MRLs considering Brazilian and European laws after 1 day for CTC and after 3 days for DOX. For OCT, this period was of 2 and 3 days according to Brazilian and European laws respectively. According to Japanese law, withdrawal time of 1, 5 and 2 days would be needed for CTC, DOX and OCT respectively. In the fluoroquinolones study, it was possible to detect traces of ENR even 9 days after treatment, which would make the export of meat to the United States and Canada infeasible. After 1 day at the last dose administrated, CIP residues were under MRLs established by Brazilian, European and Japanese laws, and after 4 days they were under limits determined by the Unites States and Canada. In the case of NOR, the withdrawal time would be of 1 day for all countries mentioned here. The results presented cooperate with the pursuit of food safety to consumers, as well as with the employment of analytical methods capable of determining drugs to comprise residue depletion studies in broilers.Dentro da cadeia produtiva de frangos de corte, antibióticos têm sido empregados no tratamento profilático e terapêutico, visando melhorar o desempenho zootécnico dos animais. Porém, o uso indiscriminado desses fármacos pode acarretar a presença de resíduos na carne e, assim, representar riscos à saúde do consumidor. Fluorquinolonas e tetraciclinas são duas classes de antibióticos amplamente utilizadas na avicultura. Para tanto, neste trabalho, desenvolveu-se e validou-se uma metodologia analítica baseada em cromatografia líquida acoplada à espectrometria de massas (LC-MS/MS), a fim de analisar resíduos de 7 antibióticos das classes citadas, em músculo de frangos. Além disso, foram realizados estudos de depleção destes fármacos em frangos de corte, a fim de quantificar os resíduos na carne. Os resultados encontrados foram comparados com os limites máximos de resíduos (LMRs) estabelecidos pelas legislações brasileira e internacionais. Como método de extração, utilizou-se um procedimento com acetonitrila acidificada e purificação por centrifugação e precipitação a baixa temperatura, sem a necessidade de utilização da etapa de extração em fase sólida (SPE). O método foi validado de acordo com a diretiva 2002/657/CE da União Europeia, avaliando parâmetros de seletividade, linearidade, especificidade, limites de detecção e quantificação, exatidão, precisão, efeito matriz, limite de decisão (CCα), capacidade de detecção (CCβ), robustez e aplicabilidade do método. Para os estudos de depleção, foram administrados, oralmente, clortetraciclina (CTC), doxiciclina (DOX) e oxitetraciclina (OTC) durante 5 dias consecutivos e ciprofloxacina (CIP), enrofloxacina (ENR) e norfloxacina (NOR) por 3 dias. Após 6, 12, 24, 48, 72, 96, 120, 144, 168, 192, 216 e 240 h da última dose administrada, foram coletadas amostras de músculo (peito) de 4 animais de cada grupo tratado e 2 do grupo controle, a fim de avaliar a concentração residual dos fármacos. O método validado apresentou-se dentro dos valores aceitáveis pela diretiva 2002/657/CE. Das 65 amostras de músculo de frango avaliadas para parâmetro de aplicabilidade, 3 apresentaram resíduos de ENR. No estudo de depleção das tetraciclinas, considerando as legislações brasileira e europeia, os resultados mostraram que foram encontrados resíduos abaixo dos LMRs após 1 dia para CTC e 3 dias para DOX. Para OTC, este período foi de 2 e 3 dias, respectivamente, de acordo com as legislações brasileira e europeia. Segundo a legislação japonesa, períodos de carência de 1, 5 e 2 dias, respectivamente, para CTC, DOX e OTC seriam necessários. No estudo das fluorquinolonas, foi possível detectar traços de ENR até 9 dias após o fim do tratamento, o que inviabilizaria a exportação desta carne para Estados Unidos e Canadá. Após 1 dia da última dose administrada, os resíduos de CIP ficaram abaixo do LMR estabelecido pelas legislações brasileira, europeia e japonesa e, após 4 dias, para Estados Unidos e Canadá. No caso da NOR, o período de carência seria de 1 dia para todos os países citados. Os resultados deste trabalho colaboram com a busca da inocuidade dos alimentos para os consumidores, bem como para a utilização de métodos analíticos capazes de serem aplicados na determinação de medicamentos a comporem estudos de depleção residual em frangos de corte.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPESporUniversidade Federal de Santa MariaCentro de Ciências RuraisPrograma de Pós-Graduação em Medicina VeterináriaUFSMBrasilMedicina VeterináriaAttribution-NonCommercial-NoDerivatives 4.0 Internationalhttp://creativecommons.org/licenses/by-nc-nd/4.0/info:eu-repo/semantics/openAccessAntibióticosResíduosValidação de metodologiaPeríodo de carênciaLimites máximos de resíduosAntibioticsAntibioticsResiduesMethod validationWithdrawal timeMaximum residue limitsCNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIAEstudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MSDepletion study of fluoroquinolones and tetracyclines in broiler chickens using LC-MS/MSinfo:eu-repo/semantics/publishedVersioninfo:eu-repo/semantics/doctoralThesisMallmann, Carlos Augustohttp://lattes.cnpq.br/5193771213666058Almeida, Carlos Alberto Araujo dehttp://lattes.cnpq.br/8218956827334831Barreto, Fabianohttp://lattes.cnpq.br/7462796814713223Rossi, Rochele Cassantahttp://lattes.cnpq.br/0627260486404735Silva, Rosselei Caiél dahttp://lattes.cnpq.br/2187197138622302http://lattes.cnpq.br/9679180542640982Silveira, Vanessa Gass da500500000007600f8b7bb02-50a2-468a-91b2-0a75e5374e2f4f84e61c-1c37-4ce5-a7b3-972b4399a73b5690e3d3-e4ff-47ee-8a96-dcb3c75bd4472fecdacb-bd48-4bc0-a3a4-8abf4956eb390cded33b-d8bb-4a1c-bc8c-a4b95841ab472faf2752-629a-4b9d-8d6e-dafb99a4efd2reponame:Manancial - Repositório Digital da UFSMinstname:Universidade Federal de Santa Maria (UFSM)instacron:UFSMORIGINALTES_PPGMV_2016_SILVEIRA_VANESSA.pdfTES_PPGMV_2016_SILVEIRA_VANESSA.pdfTese de Doutoradoapplication/pdf2028391http://repositorio.ufsm.br/bitstream/1/17600/1/TES_PPGMV_2016_SILVEIRA_VANESSA.pdf99d24b45716d66aca219085cf148837cMD51CC-LICENSElicense_rdflicense_rdfapplication/rdf+xml; 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dc.title.por.fl_str_mv |
Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS |
dc.title.alternative.eng.fl_str_mv |
Depletion study of fluoroquinolones and tetracyclines in broiler chickens using LC-MS/MS |
title |
Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS |
spellingShingle |
Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS Silveira, Vanessa Gass da Antibióticos Resíduos Validação de metodologia Período de carência Limites máximos de resíduos Antibiotics Antibiotics Residues Method validation Withdrawal time Maximum residue limits CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA |
title_short |
Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS |
title_full |
Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS |
title_fullStr |
Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS |
title_full_unstemmed |
Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS |
title_sort |
Estudo de depleção de fluorquinolonas e tetraciclinas em frangos de corte empregando LC-MS/MS |
author |
Silveira, Vanessa Gass da |
author_facet |
Silveira, Vanessa Gass da |
author_role |
author |
dc.contributor.advisor1.fl_str_mv |
Mallmann, Carlos Augusto |
dc.contributor.advisor1Lattes.fl_str_mv |
http://lattes.cnpq.br/5193771213666058 |
dc.contributor.referee1.fl_str_mv |
Almeida, Carlos Alberto Araujo de |
dc.contributor.referee1Lattes.fl_str_mv |
http://lattes.cnpq.br/8218956827334831 |
dc.contributor.referee2.fl_str_mv |
Barreto, Fabiano |
dc.contributor.referee2Lattes.fl_str_mv |
http://lattes.cnpq.br/7462796814713223 |
dc.contributor.referee3.fl_str_mv |
Rossi, Rochele Cassanta |
dc.contributor.referee3Lattes.fl_str_mv |
http://lattes.cnpq.br/0627260486404735 |
dc.contributor.referee4.fl_str_mv |
Silva, Rosselei Caiél da |
dc.contributor.referee4Lattes.fl_str_mv |
http://lattes.cnpq.br/2187197138622302 |
dc.contributor.authorLattes.fl_str_mv |
http://lattes.cnpq.br/9679180542640982 |
dc.contributor.author.fl_str_mv |
Silveira, Vanessa Gass da |
contributor_str_mv |
Mallmann, Carlos Augusto Almeida, Carlos Alberto Araujo de Barreto, Fabiano Rossi, Rochele Cassanta Silva, Rosselei Caiél da |
dc.subject.por.fl_str_mv |
Antibióticos Resíduos Validação de metodologia Período de carência Limites máximos de resíduos |
topic |
Antibióticos Resíduos Validação de metodologia Período de carência Limites máximos de resíduos Antibiotics Antibiotics Residues Method validation Withdrawal time Maximum residue limits CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA |
dc.subject.eng.fl_str_mv |
Antibiotics Antibiotics Residues Method validation Withdrawal time Maximum residue limits |
dc.subject.cnpq.fl_str_mv |
CNPQ::CIENCIAS AGRARIAS::MEDICINA VETERINARIA |
description |
Antibiotics have been widely used for prophylactic and therapeutic treatment within the broiler supply chain in order to improve animal production performance. The indiscriminate use of these drugs can, however, lead to the presence of residues in the meat and thus be a risk to the health of consumers. Fluoroquinolones and tetracyclines are two antibiotic classes that are commonly used in poultry. In this study, a liquid chromatography-based analytical method coupled with mass spectrometry was developed and validated in order to analyze residues of 7 antibiotics from the aforementioned classes in chicken muscle. Furthermore, antibiotic depletion studies were performed in broiler chickens in order to quantify the residues in the meat. The results were compared to maximum residue limits (MRLs) established by Brazilian and international laws. A procedure that employs acidified acetonitrile and purification by centrifugation and low temperature precipitation was used as the extraction method, with no need to perform a solid phase extraction (SPE) step. The method was validated in accordance with the Directive 2002/657/EC from the European Union by assessing selectivity, linearity and specificity parameters, detection and quantification limits, accuracy, precision, matrix effect, decision limit (CCα), detection capability (CCβ), robustness and applicability of the technique. For depletion studies, chlortetracycline (CTC), doxycycline (DOX) and oxytetracycline (OTC) were administered orally for 5 consecutive days and ciprofloxacin (CIP), enrofloxacin (ENR) and norfloxacin (NOR) for 3 days. After 6, 12, 24, 48, 72, 96, 120, 144, 168, 192, 216 and 240 h after the last dose, muscle samples (chest) were collected from 4 animals from each treated group and from 2 from the control group in order to assess the residual concentration of the drugs. The validated method presented values within acceptable parameters according to Directive 2002/657/EC. From 65 chicken muscle samples evaluated for the applicability parameter, 3 presented residues of ENR. In the tetracyclines depletion studies, results showed that residues were under the MRLs considering Brazilian and European laws after 1 day for CTC and after 3 days for DOX. For OCT, this period was of 2 and 3 days according to Brazilian and European laws respectively. According to Japanese law, withdrawal time of 1, 5 and 2 days would be needed for CTC, DOX and OCT respectively. In the fluoroquinolones study, it was possible to detect traces of ENR even 9 days after treatment, which would make the export of meat to the United States and Canada infeasible. After 1 day at the last dose administrated, CIP residues were under MRLs established by Brazilian, European and Japanese laws, and after 4 days they were under limits determined by the Unites States and Canada. In the case of NOR, the withdrawal time would be of 1 day for all countries mentioned here. The results presented cooperate with the pursuit of food safety to consumers, as well as with the employment of analytical methods capable of determining drugs to comprise residue depletion studies in broilers. |
publishDate |
2016 |
dc.date.issued.fl_str_mv |
2016-03-11 |
dc.date.accessioned.fl_str_mv |
2019-07-29T20:40:21Z |
dc.date.available.fl_str_mv |
2019-07-29T20:40:21Z |
dc.type.status.fl_str_mv |
info:eu-repo/semantics/publishedVersion |
dc.type.driver.fl_str_mv |
info:eu-repo/semantics/doctoralThesis |
format |
doctoralThesis |
status_str |
publishedVersion |
dc.identifier.uri.fl_str_mv |
http://repositorio.ufsm.br/handle/1/17600 |
url |
http://repositorio.ufsm.br/handle/1/17600 |
dc.language.iso.fl_str_mv |
por |
language |
por |
dc.relation.cnpq.fl_str_mv |
500500000007 |
dc.relation.confidence.fl_str_mv |
600 |
dc.relation.authority.fl_str_mv |
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dc.rights.driver.fl_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ info:eu-repo/semantics/openAccess |
rights_invalid_str_mv |
Attribution-NonCommercial-NoDerivatives 4.0 International http://creativecommons.org/licenses/by-nc-nd/4.0/ |
eu_rights_str_mv |
openAccess |
dc.publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Rurais |
dc.publisher.program.fl_str_mv |
Programa de Pós-Graduação em Medicina Veterinária |
dc.publisher.initials.fl_str_mv |
UFSM |
dc.publisher.country.fl_str_mv |
Brasil |
dc.publisher.department.fl_str_mv |
Medicina Veterinária |
publisher.none.fl_str_mv |
Universidade Federal de Santa Maria Centro de Ciências Rurais |
dc.source.none.fl_str_mv |
reponame:Manancial - Repositório Digital da UFSM instname:Universidade Federal de Santa Maria (UFSM) instacron:UFSM |
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Universidade Federal de Santa Maria (UFSM) |
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UFSM |
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UFSM |
reponame_str |
Manancial - Repositório Digital da UFSM |
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Manancial - Repositório Digital da UFSM |
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MD5 MD5 MD5 MD5 MD5 |
repository.name.fl_str_mv |
Manancial - Repositório Digital da UFSM - Universidade Federal de Santa Maria (UFSM) |
repository.mail.fl_str_mv |
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1801223692915572736 |